CN114525581B - Preparation method of double-layer 30-degree torsion angle graphene single crystal wafer - Google Patents
Preparation method of double-layer 30-degree torsion angle graphene single crystal wafer Download PDFInfo
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- CN114525581B CN114525581B CN202210129361.0A CN202210129361A CN114525581B CN 114525581 B CN114525581 B CN 114525581B CN 202210129361 A CN202210129361 A CN 202210129361A CN 114525581 B CN114525581 B CN 114525581B
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- C—CHEMISTRY; METALLURGY
- C30—CRYSTAL GROWTH
- C30B—SINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
- C30B29/00—Single crystals or homogeneous polycrystalline material with defined structure characterised by the material or by their shape
- C30B29/02—Elements
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- C—CHEMISTRY; METALLURGY
- C30—CRYSTAL GROWTH
- C30B—SINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
- C30B25/00—Single-crystal growth by chemical reaction of reactive gases, e.g. chemical vapour-deposition growth
- C30B25/02—Epitaxial-layer growth
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- C—CHEMISTRY; METALLURGY
- C30—CRYSTAL GROWTH
- C30B—SINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
- C30B25/00—Single-crystal growth by chemical reaction of reactive gases, e.g. chemical vapour-deposition growth
- C30B25/02—Epitaxial-layer growth
- C30B25/18—Epitaxial-layer growth characterised by the substrate
- C30B25/186—Epitaxial-layer growth characterised by the substrate being specially pre-treated by, e.g. chemical or physical means
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
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- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P70/00—Climate change mitigation technologies in the production process for final industrial or consumer products
- Y02P70/50—Manufacturing or production processes characterised by the final manufactured product
Abstract
The invention relates to a preparation method of a double-layer 30-degree torsion angle graphene single crystal wafer, which comprises the steps of providing a copper-nickel single crystal substrate with the thickness of 300-800nm, wherein nickel atoms in the copper-nickel single crystal substrate account for 15-22% of the total number of atoms; putting the mixture into a chemical vapor deposition furnace, and annealing the mixture at 1050-1100 ℃ in a gas atmosphere with the argon-hydrogen ratio of (100-300 sccm) to (5-15 sccm); and then growing in a gas atmosphere with the ratio of argon, hydrogen and methane of (100-300 sccm): (5-15 sccm): (0.025-0.5 sccm) and the temperature of 1050-1100 ℃ to obtain the double-layer 30-DEG torsion angle graphene single crystal wafer. According to the preparation method provided by the invention, the copper-nickel monocrystal film is used as a substrate, and the double-layer 30-degree torsion angle graphene monocrystal wafer with a large-size wafer level can be obtained by combining an annealing stage and a growth stage.
Description
Technical Field
The invention relates to preparation of graphene quasi-wafers, in particular to a preparation method of a double-layer 30-degree torsion angle graphene single crystal wafer.
Background
The graphene material has excellent photoelectric performance, and has important application in the fields of microelectronics, energy sources, biological detection and the like in the future, and is widely focused in various fields. The double-layer corner graphene has a special electronic energy band structure due to a special interlayer stacking structure, and has important potential application value in the field of microelectronics.
The current method for preparing double-layer corner graphene mainly adopts a method of growing single-layer graphene by a CVD method and then transferring and stacking for multiple times to prepare the corner graphene. The method has the advantages of complex process, low efficiency, great pollution in the transfer process, inaccurate rotation angle and limited large-scale application. At present, double-layer graphene with an AB stacking structure is mainly obtained by directly growing double-layer graphene, the size is small, the process is unstable, and batch preparation is difficult to realize.
The double-layer 30-degree torsion angle graphene reported in the current literature mainly adopts copper or platinum as a substrate, and the prepared double-layer 30-degree torsion angle graphene is small in size and low in proportion, is a polycrystalline film, and cannot meet the requirement of batch application in the future microelectronics field. For example, bing. Deng et al, ACS Nano.2020, DOI:10.1021/acsnano.9b07091, sergio Pezzini et al DOI:10.1021/acs. Nanolet.0c00172; wei Yao et al, doi/10.1073/pnas.17208255115, the resulting bilayer 30 degree twist graphene size is relatively small, ranging from several hundred microns in size. The double-layer graphene with the size is small in size and is in a local distribution state on the substrate, so that the double-layer graphene cannot be applied.
Disclosure of Invention
In order to solve the problems that the size of the double-layer 30-degree torsion angle graphene prepared in the prior art is smaller and the like, the invention provides a preparation method of a double-layer 30-degree torsion angle graphene single crystal wafer.
The preparation method of the double-layer 30-degree torsion angle graphene single crystal wafer comprises the following steps of: s1, providing a copper-nickel single crystal substrate with the thickness of 300-800nm, wherein nickel atoms in the copper-nickel single crystal substrate account for 15-22% of the total atoms; s2, placing the copper-nickel monocrystal substrate into a chemical vapor deposition furnace, and annealing at 1050-1100 ℃ in a gas atmosphere with the argon-hydrogen ratio of (100-300 sccm) (5-15 sccm) to improve crystallization quality; and then growing in a gas atmosphere with the ratio of argon to hydrogen to methane of (100-300 sccm): (5-15 sccm): (0.025-0.5 sccm) and the temperature of 1050-1100 ℃ to obtain the double-layer 30-DEG torsion angle graphene single crystal wafer, wherein each layer of graphene of the double-layer 30-DEG torsion angle single crystal graphene wafer is single crystal graphene, and the double-layer graphene forms a 30-DEG torsion angle.
The copper-nickel monocrystal substrate selected by the preparation method has a specific nickel-copper atomic ratio, so that the catalytic performance of forming graphene by catalyzing methane decomposition to generate active carbon atoms by a film and the growth of double-layer graphene can be ensured; the selected copper-nickel monocrystal substrate has a specific thickness, so that the metal film can be ensured not to be damaged in the annealing treatment and the single crystallization of the atomic-level flatness film can be ensured to be realized; the selected chemical vapor deposition has a specific gas atmosphere, so that the growth of double-layer graphene single crystals on the film can be ensured, and particularly, the alloy film can be protected from being oxidized in the annealing process, and the double-layer graphene single crystals can be grown.
Preferably, the copper-nickel single crystal substrate is a copper-nickel single crystal alloy thin film having a (111) plane. That is, the copper-nickel single crystal substrate has a (111) preferred orientation, and single crystal graphene is grown on the (111) plane.
Preferably, the purity of nickel and copper atoms in the copper-nickel single crystal substrate is 99.999%. That is, the total number of copper and nickel atoms is 99.999% of the total number of atoms of the metal thin film.
Preferably, the copper nickel single crystal substrate is a 4-8 inch sheet. It should be understood that other dimensions are also possible. 4-8 inches is a standard size commonly used in microelectronics, and 4-8 inches is chosen for future compatibility with microelectronics technologies.
Preferably, the nickel atoms in the copper-nickel single crystal substrate account for 18-20% of the total atoms.
Preferably, the thickness of the copper-nickel single crystal substrate is 500-600nm.
Preferably, the method further comprises the operation of cleaning and drying the copper-nickel single crystal substrate before the copper-nickel single crystal substrate is placed in the chemical vapor deposition furnace.
Preferably, the annealing temperature is 1070-1080 ℃.
Preferably, the annealing time is 10min-120min. In a preferred embodiment, the annealing time is 60 minutes.
Preferably, the ratio of argon, hydrogen and methane in the growth stage is (100-300 sccm): 5-15 sccm): 0.05sccm.
Preferably, the grown double-layer 30-degree torsion angle graphene single crystal wafer is integrally covered on the whole copper-nickel single crystal substrate.
According to the preparation method provided by the invention, the copper-nickel monocrystal film with the thickness of 300-800nm is adopted as the substrate, nickel atoms in the copper-nickel monocrystal substrate account for 15-22% of the total atoms, and the double-layer 30-degree torsion angle graphene monocrystal wafer with a large-size wafer level can be obtained in the combination annealing stage and the growth stage, wherein the double-layer 30-degree torsion angle graphene covers the whole substrate, and the size can reach the wafer level size (4-8 inches), so that a foundation is laid for the application of the next graphene in the microelectronics field, and the preparation method has great scientific significance and practical application value. Moreover, compared with a single-layer graphene wafer, the 30-degree torsion double-layer single-crystal graphene wafer prepared by the method has higher mechanical strength, and the transfer of graphene is easier to realize without damaging the integrity of graphene.
Drawings
FIG. 1 is a photograph of a 6 inch bilayer 30 degree twist angle graphene single crystal wafer on a copper nickel single crystal substrate obtained according to a first embodiment of the present invention;
FIG. 2 is an optical photomicrograph of bilayer 30 degree twist angle graphene obtained according to a first embodiment of the present invention;
fig. 3 is a Raman diagram of bilayer 30 degree twist angle graphene obtained according to a first embodiment of the present invention;
FIG. 4 is a LEED view of bilayer 30 degree twist angle graphene obtained in accordance with the first embodiment of the present invention;
FIG. 5 is a LEED pattern of bilayer 30 degree twist angle graphene obtained in accordance with a second embodiment of the present invention;
FIG. 6 is a LEED pattern of bilayer 30 degree twist angle graphene obtained in accordance with a third embodiment of the present invention;
FIG. 7 is a LEED pattern of bilayer 30 degree twist angle graphene obtained in accordance with a fourth embodiment of the present invention;
FIG. 8 is a LEED pattern of bilayer 30 degree twist angle graphene according to a fifth embodiment of the present invention;
FIG. 9 is a photomicrograph of a graphene/copper-nickel alloy substrate according to a first comparative example of the present invention;
fig. 10 is a Raman plot at the holes on the surface of a graphene/copper-nickel alloy substrate obtained according to a first comparative example of the present invention;
FIG. 11 is a photo-schematic diagram of a polycrystalline graphene/copper-nickel alloy substrate obtained according to a second comparative example of the present invention;
FIG. 12 is a LEED pattern of a single-layer graphene single crystal obtained according to a third comparative example of the present invention;
fig. 13 is a LEED plot of a single-layer graphene single crystal obtained according to a fourth comparative example of the present invention.
Detailed Description
Preferred embodiments of the present invention will be described in detail with reference to the accompanying drawings.
The experimental methods described in the following examples are all conventional methods unless otherwise specified; the reagents and materials, unless otherwise specified, are commercially available.
Example 1
Step a: 6 inches of copper-nickel (111) single crystal alloy film with the nickel content of 20 percent is selected, and the thickness is 500nm.
Step b: the copper-nickel monocrystal substrate is cleaned, cleaned by acetone and isopropanol, and then cleaned by a high-purity nitrogen gun.
Step c: placing the monocrystalline film into a chemical vapor deposition furnace, heating to 1080 ℃, keeping the temperature for 60min at 1080 ℃ under the condition that the ratio of argon to hydrogen is 300sccm to 5sccm, and annealing; graphene was then grown for 60min with the ratio of argon, hydrogen and methane being 300sccm to 5sccm to 0.05sccm.
Characterization of morphology:
characterization of the morphology of the double layer graphene on the resulting nickel copper (111) single crystal film was performed, wherein fig. 1 is a photograph of a double layer graphene single crystal wafer on a 6 inch copper nickel single crystal substrate surface. From this, it can be seen that a 6 inch double-layer 30 degree twist angle graphene wafer can be obtained macroscopically, i.e., a wafer-level double-layer twist angle graphene sample can be obtained; fig. 2 is an optical micrograph of the resulting bilayer graphene, from which the surface of the graphene is seen to be flat.
The quality, the number of layers and the interlayer torsion angle of the graphene of the copper-nickel (111) film are characterized:
fig. 3 is a Raman diagram of double-layer graphene on the surface of a copper-nickel single crystal substrate. The sharp peak comparison of bilayer graphene shown in the figure illustratesThe crystallinity of graphene is relatively good. At a wavenumber of 1350cm -1 No D peak was observed, indicating that the graphene quality was relatively high and free of defects.
Fig. 4 is a LEED diagram of bilayer graphene. The LEED graph shows that the graphene has a double-layer structure, the orientation of each layer of graphene is consistent and is a single crystal film, and a torsion angle of 30 degrees is formed between the two layers of graphene.
Example 2
Unlike example 1, the following is: in the copper-nickel (111) single crystal film, nickel atoms account for 22 atomic percent of copper and nickel, and the growth temperature and the annealing temperature are 1100 ℃.
Fig. 5 is a LEED diagram of bilayer graphene. The LEED graph shows that the graphene has a double-layer structure, the orientation of each layer of graphene is consistent, and an included angle of 30 degrees is formed between the two layers of graphene.
Example 3
Unlike example 1, the following is: in the copper-nickel (111) single crystal film, the percentage of nickel atoms in the copper-nickel atoms is 15%, and the growth temperature is 1050 ℃.
Fig. 6 is a LEED plot of graphene. The LEED graph shows that the graphene has a double-layer structure, the orientation of each layer of graphene is consistent, and an included angle of 30 degrees is formed between the two layers of graphene.
Example 4
Unlike example 1, the following is: the copper-nickel alloy film is 300nm, the annealing temperature and the growth temperature are 1050 ℃, the annealing time is 10min, and the ratio of hydrogen to argon in the annealing stage is 100sccm to 5sccm; the ratio of argon, hydrogen and methane in the growth stage was 100sccm to 5sccm to 0.025sccm.
Fig. 7 is a LEED diagram of the resulting bilayer graphene. The LEED graph shows 2 sets of diffraction spots which are at an angle of 30 degrees to each other, so that two layers of graphene are shown, each layer of graphene is monocrystalline graphene, and a 30-degree rotation angle is formed between the graphene layers.
Example 5
Unlike example 1, the following is: the thickness of the copper-nickel alloy film is 800nm, the annealing temperature and the growth temperature are 1100 ℃, the annealing time is 120min, and the ratio of hydrogen to argon in the annealing stage is 300sccm to 15sccm; the ratio of argon, hydrogen and methane in the growth stage was 300sccm to 15sccm to 0.5sccm.
Fig. 8 is a LEED diagram of the resulting bilayer graphene. The LEED plot shows that graphene is a bilayer structure and each layer is single crystal graphene with a 30 degree rotation angle between the graphene.
Comparative example 1
Unlike example 1, the following is: the copper-nickel alloy is 280nm.
After the annealing growth is finished, the copper-nickel alloy film is damaged, so that the graphene is also damaged, as shown in fig. 9, which is a mirror image of the copper-nickel alloy film after the high-temperature process, and the thickness holes generated by the alloy film can be clearly seen from the mirror image. Graphene is attached to the surface of an alloy film for growth, and the damage of the alloy film can also lead to the damage of the graphene on the surface of the alloy. Fig. 10 is a graphene raman plot at the hole. The raman results showed no graphene signal peaks there, indicating no graphene here. Indicating that the complete double-layer 30-degree torsion angle graphene is not obtained in the thickness range of the copper-nickel alloy film.
Comparative example 2
Unlike example 1, the copper-nickel alloy used was 850nm.
After the graphene growth process, as shown in fig. 11, a large number of polycrystalline grain boundaries are generated on the alloy surface. The graphene obtained under the thickness of copper and nickel is polycrystalline graphene and is not monocrystalline graphene with a double-layer torsion angle of 30 degrees. Furthermore, LEED also does not measure single crystal graphene images. Indicating that the double-layer torsion angle 30-degree single crystal graphene cannot be obtained in the thickness range of the copper-nickel alloy film.
Comparative example 3
Unlike example 1, the following is: the ratio of argon to hydrogen in the annealing process is 350:20, and the ratio of argon to hydrogen in the growth stage and methane is 350sccm to 20sccm to 0.6sccm.
After annealing and growth processes, the obtained graphene is single-layer single-crystal graphene, not double-side 30-degree torsion angle single-crystal graphene, as shown in fig. 12, and the LEED result shows that the graphene is a diffraction spot, which indicates that the graphene is single-layer single-crystal graphene, not double-layer 30-degree torsion angle single-crystal graphene.
Comparative example 4
Unlike example 1, the following is: the proportion of nickel atoms in the copper-nickel alloy film is 10 percent.
The result is single-layer single-crystal graphene, as shown in fig. 13, and the LEED result shows that the graphene is a diffraction spot, which indicates that the graphene is single-layer single-crystal graphene, rather than double-layer 30-degree twist angle single-crystal graphene.
The foregoing description is only a preferred embodiment of the present invention, and is not intended to limit the scope of the present invention, and various modifications can be made to the above-described embodiment of the present invention. All simple, equivalent changes and modifications made in accordance with the claims and the specification of this application fall within the scope of the patent claims. The present invention is not described in detail in the conventional art.
Claims (9)
1. The preparation method of the double-layer 30-degree torsion angle graphene single crystal wafer is characterized by comprising the following steps of:
s1, providing a copper-nickel single crystal substrate with the thickness of 300-800nm, wherein the copper-nickel single crystal substrate is a copper-nickel single crystal alloy film with a (111) surface, and nickel atoms in the copper-nickel single crystal substrate account for 15-22% of the total atoms;
s2, placing the copper-nickel monocrystal substrate into a chemical vapor deposition furnace, and annealing at 1050-1100 ℃ in a gas atmosphere with the argon-hydrogen ratio of (100-300 sccm) (5-15 sccm) to improve crystallization quality; and then growing in a gas atmosphere with the ratio of argon to hydrogen to methane of (100-300 sccm): (5-15 sccm): (0.025-0.5 sccm) and the temperature of 1050-1100 ℃ to obtain the double-layer 30-DEG torsion angle graphene single crystal wafer, wherein each layer of graphene of the double-layer 30-DEG torsion angle single crystal graphene wafer is single crystal graphene, and the double-layer graphene forms a 30-DEG torsion angle.
2. The method of producing according to claim 1, wherein the copper-nickel single crystal substrate is a 4-8 inch sheet.
3. The method of claim 1, wherein the nickel atoms in the copper-nickel single crystal substrate account for 18-20% of the total atoms.
4. The method of producing as defined in claim 1, wherein the copper-nickel single crystal substrate has a thickness of 500 to 600 a nm a.
5. The method of claim 1, further comprising the step of cleaning and drying the copper-nickel single crystal substrate before placing the copper-nickel single crystal substrate in the chemical vapor deposition furnace.
6. The method of claim 1, wherein the annealing temperature is 1070-1080 ℃.
7. The method of claim 1, wherein the annealing time is from 10min to 120min.
8. The method of claim 1, wherein the ratio of argon, hydrogen and methane in the growth stage is (100-300 sccm): 5-15 sccm): 0.05sccm.
9. The method according to claim 1, wherein the grown double-layer 30-degree twist angle graphene single crystal wafer is entirely covered on the entire copper-nickel single crystal substrate.
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